反应详情

m-Chloroperoxybenzoic acid (6.7 g, 29.9 mmol) was added in portions at 60° C. to a solution of 2-methyl-N-(3-methyl-4-nitrophenyl)acrylamide (2.9 g, 13.2 mmol) and 2,6-di-tert-butyl-4-methylphenol (66 mg) in 1,2-dichloroethane (80 ml). The string was continued at 60° C. for 6 h, and the reaction mixture was allowed to cool to room temperature. The precipitated m-chlorobenzoic acid was filtered, and the filtrate was extracted with 1 M Na2CO3 (4×60 ml). The organic phase was dried over Na2SO4 and evaporated. The yield was 3.05 g. 1H NMR (DMSO-d6): 1.54 (3H, s), 2.51 (3H, s), 2.99 (1H, d, J=5.1 Hz), 3.05 (1H, d, J=5.1 Hz), 7.79 (2H, m), 8.01 (1H, m), 9.98 (1H, s).

1. filtrationThe precipitated m-chlorobenzoic acid was filtered
2. extractionthe filtrate was extracted with 1 M Na2CO3 (4×60 ml)
3. dry with materialThe organic phase was dried over Na2SO4
4. customevaporated